JP2010505230A - Metal paste for conductive film formation - Google Patents
Metal paste for conductive film formation Download PDFInfo
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- JP2010505230A JP2010505230A JP2009530245A JP2009530245A JP2010505230A JP 2010505230 A JP2010505230 A JP 2010505230A JP 2009530245 A JP2009530245 A JP 2009530245A JP 2009530245 A JP2009530245 A JP 2009530245A JP 2010505230 A JP2010505230 A JP 2010505230A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0242—Shape of an individual particle
- H05K2201/0245—Flakes, flat particles or lamellar particles
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/12—Using specific substances
- H05K2203/121—Metallo-organic compounds
Abstract
本発明は導電膜形成のための金属ペーストに関するものであって、ヘテロ原子Ｐ、Ｓ、ＯまたはＮを有する反応性有機溶媒に溶解された金属溶液；金属粉末；バインダー；及び粘度調節用極性または非極性溶媒残量で構成される導電膜形成用ペーストを提供する。
本発明の金属ペースト組成物を用いると従来のペーストで形成された伝導性パターンと比較して相対的に薄い厚さまたは狭い線幅でもはるかに低い電気抵抗の特性を示し、高価なナノスケールの金属粒子を用いなくても非常に低い温度で熱処理が可能である、良好な微細構造を有する導電膜を得ることができる。特に本発明の金属ペーストは銀ペーストを提供し、この銀ペーストは経済的に製造でき、さまざまな表面に適用できる。
【選択図】図２The present invention relates to a metal paste for forming a conductive film, and includes a metal solution dissolved in a reactive organic solvent having a heteroatom P, S, O, or N; a metal powder; a binder; Provided is a conductive film forming paste comprising a non-polar solvent remaining amount.
The metal paste composition of the present invention exhibits much lower electrical resistance characteristics even at relatively thin thicknesses or narrow line widths compared to conductive patterns formed with conventional pastes, and is an expensive nanoscale A conductive film having a good microstructure that can be heat-treated at a very low temperature without using metal particles can be obtained. In particular, the metal paste of the present invention provides a silver paste that can be produced economically and applied to a variety of surfaces.
[Selection] Figure 2
Description
本発明は導電膜形成のための金属ペーストに関する。ＬＣＤ（液晶ディスプレイ）とＰＤＰ（プラズマディスプレイパネル）のような平板ディスプレイの導電線パターン形成、及びタッチスクリーンの電極部、面発光バックライト（ＦＦＬ）のＰＡＤ部電極、フレキシブルＰＣＢの電極部やＲＦＩＤのアンテナ等に導電膜が用いられる。 The present invention relates to a metal paste for forming a conductive film. Conductive line pattern formation for flat panel displays such as LCD (Liquid Crystal Display) and PDP (Plasma Display Panel), touch screen electrode part, surface emission backlight (FFL) PAD part electrode, flexible PCB electrode part and RFID A conductive film is used for an antenna or the like.
半導体やディスプレイに適用されるパターン形成技術は大別して３種に分けられる。第一に、薄膜形成技術に主に適用される減法（ｓｕｂｔｒａｃｔｉｖｅ；成膜をした後リソグラフィでパターンを現像した後エッチングして製造）、第二に、スクリーン印刷方式のような厚膜形成技術に主に適用される加法（ａｄｄｉｔｉｖｅ；スクリーンプリンティングのような接触印刷方式によるパターン形成）と第三に、これらを併用する加減法に分けることができる。 Pattern forming techniques applied to semiconductors and displays are roughly divided into three types. First, subtractive (mainly applied to thin film formation technology; manufacturing by etching after developing a pattern after forming a film), and second, thick film formation technology such as screen printing. Addition (additive; pattern formation by a contact printing method such as screen printing) which is mainly applied and thirdly, an addition and subtraction method using these in combination can be divided.
ディスプレイに適用される導電性パターンの形成は主に加法であって、接触または非接触印刷方式によって、基板の種類と使用目的によって適切なインクまたはペーストを一定なパターンで形成して後処理して、基板上に固定する過程を経る。場合によって、エッチングを付加する加減法が採用されることもある。 The formation of conductive patterns applied to displays is mainly additive. After contact processing or non-contact printing, an appropriate ink or paste is formed in a certain pattern according to the type of substrate and purpose of use, and then post-processed. , Through the process of fixing on the substrate. In some cases, a method of adding or subtracting etching may be employed.
ベスト（Ｖｅｓｔ、Ｒ．Ｗ．）がＭＯＤ物質を用いてインクの製造可能性を試験した（ＩＥＥＥ Ｔｒａｎｓａｃｔｉｏｎｓ ｏｎ Ｃｏｍｐｏｎｅｎｔｓ、Ｈｙｂｒｉｄｓ ａｎｄ Ｍａｍｕｆａｃｔｕｒｉｎｇ Ｔｅｃｈｎｏｌｏｇｙ、１２（４）、５４５−５４９、１９８７）以来、ＭＯＤ物質を用いるパターン形成用インクに対して多くの研究がなされた。 Since Best (R.W.) has tested the manufacturability of inks using MOD materials (IEEE Transactions on Components, Hybrids and Manufacturing Technology, 12 (4), 545-549, 1987) Much research has been done on the patterning inks used.
ここでＭＯＤ（ｍｅｔａｌｌｏ−ｏｒｇａｎｉｃ ｄｅｃｏｍｐｏｓｉｔｏｎ）物質とは有機金属化合物で金属溶融温度より低い温度で分解されて金属化される化合物をいう。 Here, a MOD (metallo-organic decomposition) substance is an organic metal compound that is decomposed at a temperature lower than the metal melting temperature to be metallized.
コビオ社（Ｋｏｖｉｏ、Ｉｎｃ）の米国特許６８７８１８４号にＭＯＤと還元剤（例えば、アルデヒド）を用いてナノパーティクル状のインクを形成する技術を開示している。しかし、この技術では反応条件が難しく、高価なＭＯＤ物質を大量に用いなければならない。また形成されたナノパーティクル状の粒子では十分な電気伝導性を得ることができない。 US Pat. No. 6,878,184 to Kobio, Inc. discloses a technique for forming nanoparticulate inks using MOD and a reducing agent (eg, aldehyde). However, with this technique, the reaction conditions are difficult and a large amount of expensive MOD material must be used. Moreover, sufficient electrical conductivity cannot be obtained with the formed nanoparticle-like particles.
前記ＭＯＤインクとナノパーティクルを懸濁して用いるインクは比較的低い金属化温度を達成することはできるが、高価で、バルク金属に比べて電気伝導性が著しく低下するという問題点がある。 The MOD ink and the ink using nanoparticles suspended therein can achieve a relatively low metallization temperature, but are expensive and have a problem that the electric conductivity is remarkably reduced as compared with bulk metal.
バルク金属が有する高い電気伝導性と低温金属化が可能なＭＯＤの長所を組み合わせて、キド（Ｋｙｄｄ）その他の国際公開ＷＯ９８−３７１３３は、ＭＯＤ物質と粒子性金属の複合組成物をスクリーン印刷用インクで用いることを開示している。しかし前記特許では、プラスチック基板に用いることができるように十分低い温度で金属化する印刷用インクを提示できなくなっている。また、ＭＯＤ物質と粒子性金属は粒子状態であるため、インクで製造するためにはこれらと共にビヒクルをボールミルによって微細に粉砕して混合しなければならない別途の製造工程が必要である。またこのようなインクの製造は現場適応性が非常に低く、製造社であらかじめ製造された通り用いなければならない等の問題点がある。 Combining the high electrical conductivity of bulk metals with the advantages of MOD capable of low temperature metallization, Kydd et al., International Publication WO 98-37133, discloses a composite composition of MOD material and particulate metal for screen printing inks. Is used. However, the patent fails to present printing inks that metallize at a sufficiently low temperature so that they can be used on plastic substrates. In addition, since the MOD substance and the particulate metal are in a particle state, a separate manufacturing process is required in which the vehicle must be finely pulverized and mixed with a ball mill together with these. In addition, the production of such an ink has a very low site adaptability and has a problem that it must be used as it is manufactured in advance by a manufacturer.
本発明の目的は電気伝導性が優秀な導電膜形成のための金属ペーストを提供することである。 An object of the present invention is to provide a metal paste for forming a conductive film having excellent electrical conductivity.
また、本発明の目的は非常に低い低温焼成条件で優秀な電気伝導性を有しながら、経済的に製造可能でさまざまな表面に適用性が高い銀ペーストを提供することである。 Another object of the present invention is to provide a silver paste that can be produced economically and has high applicability to various surfaces while having excellent electrical conductivity under very low temperature firing conditions.
本発明によって、ヘテロ原子Ｐ、Ｓ、ＯまたはＮを有する反応性有機溶媒に溶解された金属溶液；金属粉末；バインダー；及び粘度調節用極性または非極性溶媒残量で構成される導電膜形成用ペーストが提供される。前記ヘテロ原子Ｐ、Ｓ、ＯとＮを有する反応性有機溶媒はケトン基、メルカプト基、カルボキシル基、アニリン基、エーテル基または亜硫酸基等を有して特定金属とキレートまたは錯体を形成する有機溶媒である。 According to the present invention, a metal solution dissolved in a reactive organic solvent having a heteroatom P, S, O, or N; a metal powder; a binder; and a conductive film formed of a viscosity-adjusting polar or nonpolar solvent residue A paste is provided. The reactive organic solvent having heteroatoms P, S, O and N is an organic solvent having a ketone group, a mercapto group, a carboxyl group, an aniline group, an ether group or a sulfite group and forming a chelate or complex with a specific metal. It is.
また、本発明によって、１〜３のカルボキシル基を有する炭素数０〜１２の脂肪族カルボキシ化（今後"脂肪酸"）金属有効量と前記脂肪酸金属を溶解する反応性有機溶媒で構成される金属溶液；金属粉末；熱硬化性バインダー；及び粘度調節用極性または非極性溶媒残量で構成される導電膜形成用ペーストが提供される。前記反応性有機溶媒は前記脂肪酸金属を溶解して溶液状態にする。前記反応性有機溶媒はヘテロ原子Ｐ、Ｓ、ＯとＮを有する溶媒でケトン基、メルカプト基、カルボキシル基、アニリン基、エーテル基または亜硫酸基を有する有機溶媒である。 Further, according to the present invention, a metal solution composed of an effective amount of an aliphatic carboxylated (hereinafter “fatty acid”) metal having 1 to 3 carboxyl groups and a reactive organic solvent that dissolves the fatty acid metal. A conductive film forming paste comprising: a metal powder; a thermosetting binder; and a residual polar or nonpolar solvent for viscosity adjustment. The reactive organic solvent dissolves the fatty acid metal into a solution state. The reactive organic solvent is a solvent having heteroatoms P, S, O and N, and is an organic solvent having a ketone group, mercapto group, carboxyl group, aniline group, ether group or sulfite group.
前記金属は例えば、銀、鉄、亜鉛、スズ、ニッケル、インジウム、金、白金、パラジウム、鉛、アンチモン、銅またはこれらの合金であるが、これらに制限されない。前記金属溶液と前記金属粉末は相異なる金属であることができるが、好ましくは同じ金属である。前記金属溶液は、好ましくは０．１〜９０重量％、最も好ましくは０．１〜４０重量％であって、前記金属粉末は、好ましくは１〜９５重量％、最も好ましくは１〜６５重量％である。前記銀粉末の平均粒径は、好ましくはマイクロメーター単位で、例えば、０．１ないし１０マイクロメーターの範囲で、最も好ましくは１ないし５マイクロメーター範囲である。 Examples of the metal include, but are not limited to, silver, iron, zinc, tin, nickel, indium, gold, platinum, palladium, lead, antimony, copper, and alloys thereof. The metal solution and the metal powder may be different metals, but are preferably the same metal. The metal solution is preferably 0.1 to 90 wt%, most preferably 0.1 to 40 wt%, and the metal powder is preferably 1 to 95 wt%, most preferably 1 to 65 wt%. It is. The average particle size of the silver powder is preferably in units of micrometers, for example, in the range of 0.1 to 10 micrometers, and most preferably in the range of 1 to 5 micrometers.
本発明の金属ペースト組成物は金属インク、すなわち有機金属溶液を金属ペーストのビヒクルで用いることに特徴がある。従来の金属粉末＋ビヒクルでなったペーストより低温金属化が可能であって、また従来の金属粉末＋ＭＯＤ粉末の混合ボールミル粉砕物より製造するのが容易である。これを概略的に説明すると次の図のとおりである。
The metal paste composition of the present invention is characterized in that a metal ink, that is, an organic metal solution is used in a metal paste vehicle. It can be metallized at a lower temperature than a paste made of conventional metal powder + vehicle, and can be easily manufactured from a mixed ball mill pulverized product of conventional metal powder + MOD powder. This is schematically shown in the following figure.
本発明の金属ペーストは金属が溶液に懸濁されていることを意味し、多様な粘度を使用目的によって選定することができる。このような金属ペーストは粘度を調節し、適切なバインダーを添加して、多様な印刷方法、例えば、グラビア、フレキソ印刷、スクリーン、ロータリー、ディスペンサー、オフセットに適用されることができる。コーティング可能な粘度は１〜７０，０００ｃＰｓである。シルクスクリーン印刷の場合１０，０００〜３５，０００ｃＰｓであって、好ましくは１０，０００〜２０，０００ｃＰｓである。 The metal paste of the present invention means that the metal is suspended in the solution, and various viscosities can be selected depending on the purpose of use. Such metal paste can be applied to various printing methods such as gravure, flexographic printing, screen, rotary, dispenser, offset by adjusting viscosity and adding appropriate binder. The coatable viscosity is 1 to 70,000 cPs. In the case of silk screen printing, it is 10,000 to 35,000 cPs, and preferably 10,000 to 20,000 cPs.
前記バインダーは広くは天然、合成高分子またはこれらの混合物である。例えば、ロジン配合物、ウレタン系、アクリル系とエポキシ樹脂系列の熱硬化性バインダー等が用いられることができるが、一般的に０．１〜１５重量％、好ましくは１〜１３重量％用いられる。１５重量％を越えれば伝導性が不良になって、０．１重量％未満ならば結合力が低下する。
好ましくは前記金属は特に銀である。本発明によって、好ましい実施例で、１〜３のカルボキシル基を有する炭素数１〜１２の脂肪酸銀有効量と銀とキレート剤または錯体を形成する反応性有機溶媒で構成される銀溶液０．１〜９０重量％；銀粉末１〜６０重量％；熱硬化性バインダー１〜１３重量％；及び粘度調節用極性または非極性溶媒残量で構成される導電膜形成用ペーストが提供される。
The binder is broadly a natural, synthetic polymer or a mixture thereof. For example, rosin compounds, urethane-based, acrylic-based and epoxy resin-based thermosetting binders can be used, but generally 0.1 to 15% by weight, preferably 1 to 13% by weight. If it exceeds 15% by weight, the conductivity is poor, and if it is less than 0.1% by weight, the bonding strength is lowered.
Preferably the metal is in particular silver. According to the present invention, in a preferred embodiment, a silver solution 0.1 composed of an effective amount of silver salt of 1 to 12 carbon atoms having 1 to 3 carboxyl groups and a reactive organic solvent that forms a chelating agent or complex with silver. There is provided a paste for forming a conductive film comprising: -90 wt%; silver powder 1-60 wt%; thermosetting binder 1-13 wt%; and viscosity-adjusting polar or nonpolar solvent residue.
本発明の脂肪酸銀は直鎖または分枝状であってアミノ基、ニトロ基またはヒドロキシ基によって置換されることができる。前記反応性有機溶媒は、望ましくは、炭素数１〜６の脂肪族またはヒドロキシ基を有する脂肪族で一つ以上置換されたアミンと炭素数１〜１６の直鎖または分枝状の脂肪族チオールで構成される群から選択される。前記脂肪酸銀は、好ましくは飽和された、または二重結合を一個または二個を有する脂肪酸銀である。例えば、マレイン酸銀、マロン酸銀、コハク酸銀、酢酸銀、リンゴ酸銀、メタクリル酸銀、プロピオン酸銀、ソルビン酸銀、クエン酸銀、ウンデシレン酸銀、ネオデカン酸銀、オレイン酸銀、シュウ酸銀、ギ酸銀、グルコン酸銀またはこれらの混合物であって、好ましくはクエン酸銀、シュウ酸銀、ギ酸銀、マレイン酸銀またはこれらの混合物である。 The fatty acid silver of the present invention is linear or branched and can be substituted by an amino group, a nitro group or a hydroxy group. Preferably, the reactive organic solvent is an amine substituted with one or more aliphatic having 1 to 6 carbon atoms or an aliphatic group having a hydroxy group, and a linear or branched aliphatic thiol having 1 to 16 carbon atoms. Selected from the group consisting of The fatty acid silver is preferably fatty acid silver which is saturated or has one or two double bonds. For example, silver maleate, silver malonate, silver succinate, silver acetate, silver malate, silver methacrylate, silver propionate, silver sorbate, silver citrate, silver undecylate, silver neodecanoate, silver oleate, silver Silver acid silver, silver formate, silver gluconate or a mixture thereof, preferably silver citrate, silver oxalate, silver formate, silver maleate or a mixture thereof.
前記銀溶液は好ましくは０．１〜４０重量％の範囲である。 The silver solution is preferably in the range of 0.1 to 40% by weight.
前記銀粉末の平均粒径は、好ましくはマイクロメーター単位で、例えば、０．１ないし１０マイクロメーターの範囲で、最も好ましくは１ないし５マイクロメーター範囲である。前記銀粉末の形態は好ましくは板状である。 The average particle size of the silver powder is preferably in units of micrometers, for example, in the range of 0.1 to 10 micrometers, and most preferably in the range of 1 to 5 micrometers. The silver powder is preferably plate-shaped.
前記反応性有機溶媒は、好ましくはメチルアミン、エチルアミン、イソプロピルアミン、モノエタノールアミン、ジエタノールアミン、トリエタノールアミンまたは炭素数５ないし１４の直鎖状の飽和脂肪族チオールであって、最も好ましくはエチルアミンである。 The reactive organic solvent is preferably methylamine, ethylamine, isopropylamine, monoethanolamine, diethanolamine, triethanolamine or a linear saturated aliphatic thiol having 5 to 14 carbon atoms, most preferably ethylamine. is there.
前記極性または非極性溶媒は、１ないし３価のヒドロキシ基を有する炭素数１ないし４の脂肪族アルコール、前記アルコールとの炭素数２ないし８のアルキルエーテル、または前記アルコールとの炭素数２ないし８のアルキルエステルで、例えば、ブチルカルビトールアセテート、ブチルカルビトール、エチルカルビトール、エチルカルビトールアセテート、テルピネオール、テキサノール、メントール、イソアミルアセテート、メタノール、エタノールとこれらの混合物で構成される群から選択される。 The polar or nonpolar solvent is an aliphatic alcohol having 1 to 4 carbon atoms having a monovalent to trivalent hydroxy group, an alkyl ether having 2 to 8 carbon atoms with the alcohol, or 2 to 8 carbon atoms with the alcohol. Alkyl ester of, for example, selected from the group consisting of butyl carbitol acetate, butyl carbitol, ethyl carbitol, ethyl carbitol acetate, terpineol, texanol, menthol, isoamyl acetate, methanol, ethanol and mixtures thereof .
本発明による金属ペースト組成物は、既存の金属ペーストと比較してはるかに緻密な微細構造を有していて、既存のペーストで形成された伝導性パターンと比較して相対的に薄い厚さまたは狭い線幅でもはるかに低い電気抵抗の特性を示し、高価なナノスケールの金属粒子を用いなくても非常に低い温度で熱処理が可能であるという長所を提供する。また、本発明の銀ペーストは経済的に製造可能で多様な表面に高い適応性を示す。 The metal paste composition according to the present invention has a much denser microstructure compared to existing metal pastes and has a relatively thin thickness or compared to the conductive pattern formed with the existing pastes. Even with a narrow line width, it exhibits a much lower electrical resistance characteristic and offers the advantage that it can be heat treated at very low temperatures without the use of expensive nanoscale metal particles. In addition, the silver paste of the present invention can be produced economically and exhibits high adaptability to various surfaces.
本発明の銀ペーストはガラス基板、ＰＥＴのようなプラスチック基板、特にフレキシブルＰＣＢの基板で用いられるポリイミド基板に適用可能であって、次世代フレキシブルディスプレイ、タッチパネル、フレキシブルＰＣＢ、ＲＦＩＤ等に応用され、これらの生産工程と費用を減らすことができる。 The silver paste of the present invention can be applied to glass substrates, plastic substrates such as PET, particularly polyimide substrates used in flexible PCB substrates, and can be applied to next-generation flexible displays, touch panels, flexible PCBs, RFIDs, etc. Can reduce the production process and cost.
以下本発明を実施例によって詳細に説明する。このような実施例は本発明を例示するためのもので本発明の保護範囲を制限するものと解釈されてはならない。これら実施例で、板状銀粉末は直径が厚さの５０倍であって、平均粒径が３マイクロメーターである板状銀粉末を用いる。また、これら実施例で、熱硬化性バインダーでは二液型エポキシ系列のレジン成分でＫｕｍｈｏＰ＆Ｂ化学のＫＥＲ３００１（商品名）と硬化剤でアルドリッチ社の２−エチルイミダゾールを９５：５容量配合比で用いた。また、実施例で脂肪酸銀溶液がそれぞれ２、４、６、１０、１６と２０重量％になるように添加した。ここで銀インクとは銀溶液と同じ意味で用いられる。
〔比較例１〕
板状銀粉末（直径が厚さの５０倍であって平均粒径が３マイクロメーター）６０ｇと、ノーマルテルピネオール１４．３８ｇと、ブチルカルビトールアセテート２．５ｇと、エタノール残量で構成された１００ｇペースト組成物を完全に混合してペースト組成物を作った。前記ペースト組成物をガラス基板上にコーティングして、１３０°Ｃ、２００°Ｃ、２５０°Ｃで熱処理し、２−プローブ装置で線抵抗を測定して表１に表示した．２００°Ｃでガラス基板上にコーティングされた銀膜は、既存のペーストと比較するために切断して断面及び表面をＳＥＭで観察し、そのイメージを図１に表示した。
Hereinafter, the present invention will be described in detail by way of examples. Such examples are intended to illustrate the invention and should not be construed to limit the scope of protection of the invention. In these examples, a plate-like silver powder having a diameter 50 times the thickness and an average particle size of 3 micrometers is used. In these examples, the thermosetting binder used was a two-component epoxy series resin component, KumhoP & B Chemical's KER3001 (trade name), and a curing agent, Aldrich 2-ethylimidazole, in a 95: 5 volume ratio. . Moreover, it added so that a fatty-acid silver solution might be 2, 4, 6, 10, 16, and 20 weight% in an Example, respectively. Here, the silver ink is used in the same meaning as the silver solution.
[Comparative Example 1]
60 g of plate-like silver powder (50 times the diameter and average particle size is 3 micrometers), 14.38 g of normal terpineol, 2.5 g of butyl carbitol acetate, and 100 g of ethanol remaining The paste composition was mixed thoroughly to make a paste composition. The paste composition was coated on a glass substrate, heat-treated at 130 ° C., 200 ° C. and 250 ° C., and the line resistance was measured with a 2-probe device and displayed in Table 1. The silver film coated on the glass substrate at 200 ° C. was cut for comparison with the existing paste, the cross section and the surface were observed with SEM, and the image was displayed in FIG.
５０ｍｍｏｌのギ酸を５０ｍＬのメタノールに解離させる。撹はんされているこの溶液に５０ｍｍｏｌのＮａＯＨが解離されている５０ｍＬの水をゆっくり添加して、ギ酸ナトリウムを形成させる。この溶液に５０ｍｍｏｌの硝酸銀が解離されている５０ｍＬの水を添加させれば白色沈殿が迅速に形成される。この沈殿物を水で十分に洗浄した次に濾過して、再びメタノールで十分に洗浄して常温で乾燥してギ酸銀を製造する。 Dissociate 50 mmol of formic acid into 50 mL of methanol. To this stirred solution is slowly added 50 mL of water in which 50 mmol of NaOH is dissociated to form sodium formate. If 50 mL of water from which 50 mmol of silver nitrate is dissociated is added to this solution, a white precipitate is rapidly formed. The precipitate is washed thoroughly with water, then filtered, washed again with methanol and dried at room temperature to produce silver formate.
前記ギ酸銀０．１ｍｏｌを０．１２ｍｏｌのエチルアミンで完全に溶解させた次に、メタノールで全体重量が５０ｇになるように調節した。続いて３０分間十分に撹はんして完全に透明なギ酸銀インクを製造した。 Next, 0.1 mol of the silver formate was completely dissolved with 0.12 mol of ethylamine, and the total weight was adjusted to 50 g with methanol. Subsequently, the mixture was sufficiently stirred for 30 minutes to produce a completely transparent silver formate ink.
前記製造されたギ酸銀インク２ｇを平均粒子サイズが３μｍである板状銀粉末５９．４ｇとノーマルテルピネオール１４．４ｇとブチルカルビトールアセテート２．５ｇ、エポキシ樹脂バインダー４ｇとエタノール残量で構成された１００ｇペースト組成物に入れて完全に混合してペースト組成物を作った。 2 g of the prepared silver formate ink was composed of 59.4 g of plate-like silver powder having an average particle size of 3 μm, 14.4 g of normal terpineol, 2.5 g of butyl carbitol acetate, 4 g of epoxy resin binder and the remaining amount of ethanol. A 100 g paste composition was mixed thoroughly to make a paste composition.
前記ペースト組成物をガラス基板、ＰＥＴ基板、またはポリイミド基板上にスクリーンプリンティングして、各々１３０°Ｃ、２００°Ｃ、２５０°Ｃで熱処理し、２−プローブ装置で線抵抗を測定して特性化した。別途にガラス基板上にコーティングされた銀膜は既存のペーストと比較するために切断して断面及び表面をＳＥＭで観察した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 The paste composition is screen-printed on a glass substrate, PET substrate, or polyimide substrate, heat-treated at 130 ° C, 200 ° C, and 250 ° C, respectively, and measured by a 2-probe device to measure line resistance. did. Separately, the silver film coated on the glass substrate was cut for comparison with the existing paste, and the cross section and the surface were observed with SEM. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
実施例１で製造されたギ酸銀インクを用いた。ギ酸銀インク４ｇと板状銀粉末５８．８ｇを用いることを除いては実施例１と同じく実施してペースト組成物を作って実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 The silver formate ink prepared in Example 1 was used. A paste composition was prepared in the same manner as in Example 1 except that 4 g of silver formate ink and 58.8 g of plate-like silver powder were used. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
実施例１で製造されたギ酸銀を用いた。ギ酸銀インク６ｇと板状銀粉末５８．２ｇを用いることを除いては実施例１と同じく実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 The silver formate prepared in Example 1 was used. The same procedure as in Example 1 was performed except that 6 g of silver formate ink and 58.2 g of plate-like silver powder were used. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
実施例１で製造されたギ酸銀を用いた。ギ酸銀インク１０ｇと板状銀粉末５７ｇを用いることを除いては実施例１と同じく実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 The silver formate prepared in Example 1 was used. The same procedure as in Example 1 was performed except that 10 g of silver formate ink and 57 g of plate-like silver powder were used. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
実施例１で製造されたギ酸銀を用いた。ギ酸銀インク１６ｇと板状銀粉末５５．２ｇを用いることを除いては実施例１と同じく実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 The silver formate prepared in Example 1 was used. The same procedure as in Example 1 was performed except that 16 g of silver formate ink and 55.2 g of plate-like silver powder were used. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
実施例１で製造されたギ酸銀を用いた。ギ酸銀インク２０ｇと板状銀粉末５４ｇを用いることを除いては実施例１と同じく実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 The silver formate prepared in Example 1 was used. The same procedure as in Example 1 was performed except that 20 g of silver formate ink and 54 g of plate-like silver powder were used. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
ギ酸の代わりにシュウ酸を用いることを除いて実施例１と同じ方法でシュウ酸銀インクを製造する。前記製造されたシュウ酸銀インク２ｇと板状銀粉末５９．４ｇを用いることを除いては実施例１と同じくペースト組成物を作って実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表１に整理した。 A silver oxalate ink is produced in the same manner as in Example 1 except that oxalic acid is used instead of formic acid. A paste composition was prepared and carried out in the same manner as in Example 1 except that 2 g of the prepared silver oxalate ink and 59.4 g of plate-like silver powder were used. Table 1 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
シュウ酸銀インク４ｇと板状銀粉末５８．８ｇを用いることを除いては実施例７と同じく実施した。 The same procedure as in Example 7 was performed except that 4 g of silver oxalate ink and 58.8 g of plate-like silver powder were used.
シュウ酸銀インク６ｇと板状銀粉末５８．２ｇを用いることを除いては実施例７と同じく実施した。 The same procedure as in Example 7 was performed except that 6 g of silver oxalate ink and 58.2 g of plate-like silver powder were used.
シュウ酸銀インク１０ｇと板状銀粉末５７ｇを用いることを除いては実施例７と同じく実施した。特に２００°Ｃで熱処理されたガラス基板上塗膜の断面及び表面のＳＥＭイメージを図２に例示した。図１よりはるかに緻密な構造を有していることを示す。図３、図４と図５はそれぞれガラス基板、ＰＥＴ基板、またはポリイミド基板上に前記ペーストをスクリーンプリンティングして２００°Ｃで熱処理した後の写真を示す。 The same procedure as in Example 7 was performed except that 10 g of silver oxalate ink and 57 g of plate-like silver powder were used. The SEM image of the cross section and the surface of the coating film on the glass substrate heat-treated especially at 200 ° C. is illustrated in FIG. It shows that it has a much denser structure than FIG. 3, 4 and 5 are photographs after the paste is screen printed on a glass substrate, a PET substrate or a polyimide substrate and heat-treated at 200 ° C., respectively.
シュウ酸銀インク１６ｇと板状銀粉末５５．２ｇを用いることを除いては実施例７と同じく実施した。 The same procedure as in Example 7 was performed except that 16 g of silver oxalate ink and 55.2 g of plate-like silver powder were used.
シュウ酸銀インク２０ｇと板状銀粉末５４ｇを用いることを除いては実施例７と同じく実施した。 The same procedure as in Example 7 was performed except that 20 g of silver oxalate ink and 54 g of plate-like silver powder were used.
ギ酸の代わりにクエン酸を用いることを除いて実施例１と同じ方法でクエン酸銀インクを製造する。前記製造されたクエン酸銀インク２ｇと板状銀粉末５９．４ｇを用いることを除いては実施例１と同じくペースト組成物を作って実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表２に整理した。 A silver citrate ink is prepared in the same manner as in Example 1 except that citric acid is used instead of formic acid. A paste composition was prepared and carried out in the same manner as in Example 1 except that 2 g of the prepared silver citrate ink and 59.4 g of plate-like silver powder were used. Table 2 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
クエン酸銀インク４ｇと板状銀粉末５８．８ｇを用いることを除いては実施例１３と同じく実施した。 The same operation as in Example 13 was performed except that 4 g of silver citrate ink and 58.8 g of plate-like silver powder were used.
クエン酸銀インク６ｇと板状銀粉末５８．２ｇを用いることを除いては実施例１３と同じく実施した。 The same procedure as in Example 13 was performed except that 6 g of silver citrate ink and 58.2 g of plate-like silver powder were used.
クエン酸銀インク１０ｇと板状銀粉末５７ｇを用いることを除いては実施例１３と同じく実施した。 The same operation as in Example 13 was performed except that 10 g of silver citrate ink and 57 g of plate-like silver powder were used.
クエン酸銀インク１６ｇと板状銀粉末５５．２ｇを用いることを除いては実施例１３と同じく実施した。 The same procedure as in Example 13 was performed except that 16 g of silver citrate ink and 55.2 g of plate-like silver powder were used.
クエン酸銀インク２０ｇと板状銀粉末５４ｇを用いることを除いては実施例１３と同じく実施した。 The same procedure as in Example 13 was performed except that 20 g of silver citrate ink and 54 g of plate-like silver powder were used.
ギ酸の代わりにリンゴ酸を用いることを除いて実施例１と同じ方法でリンゴ酸銀インクを製造する。前記製造されたリンゴ酸銀インク２ｇと板状銀粉末５９．４ｇを用いることを除いては実施例１と同じくペースト組成物を作って実施した。塗膜の粘度、熱処理された塗膜の接着力と電気抵抗は表２に整理した。 A silver malate ink is produced in the same manner as in Example 1 except that malic acid is used instead of formic acid. A paste composition was prepared and carried out in the same manner as in Example 1 except that 2 g of the prepared silver malate ink and 59.4 g of plate-like silver powder were used. Table 2 shows the viscosity of the coating film, the adhesive strength and the electrical resistance of the heat-treated coating film.
リンゴ酸銀インク４ｇと板状銀粉末５８．８ｇを用いることを除いては実施例１９と同じく実施した。 The same procedure as in Example 19 was performed except that 4 g of silver malate ink and 58.8 g of plate-like silver powder were used.
リンゴ酸銀インク６ｇと板状銀粉末５８．２ｇを用いることを除いては実施例１９と同じく実施した。 The same operation as in Example 19 was performed except that 6 g of silver malate ink and 58.2 g of plate-like silver powder were used.
リンゴ酸銀インク１０ｇと板状銀粉末５７ｇを用いることを除いては実施例１９と同じく実施した。 The same procedure as in Example 19 was performed except that 10 g of silver malate ink and 57 g of plate-like silver powder were used.
リンゴ酸銀インク１６ｇと板状銀粉末５５．２ｇを用いることを除いては実施例１９と同じく実施した。 The same procedure as in Example 19 was performed except that 16 g of silver malate ink and 55.2 g of plate-like silver powder were used.
リンゴ酸銀インク２０ｇと板状銀粉末５４ｇを用いることを除いては実施例１９と同じく実施した。 The same operation as in Example 19 was performed except that 20 g of silver malate ink and 54 g of plate-like silver powder were used.
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| KR1020070009177A KR100709724B1 (en) | 2007-01-30 | 2007-01-30 | Metal paste for forming conductive layers |
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| PCT/KR2007/002561 WO2008093915A1 (en) | 2007-01-30 | 2007-05-28 | A metal paste for forming a conductive layer |
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| JP2005183144A (en) * | 2003-12-18 | 2005-07-07 | Alps Electric Co Ltd | Conductive composition and manufacturing method of same |
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| KR100196399B1 (en) * | 1996-05-07 | 1999-06-15 | 조희재 | Composites of conductive paste |
| KR19990056608A (en) * | 1997-12-29 | 1999-07-15 | 조희재 | Thick Film Conductor Paste Composition |
| KR100637174B1 (en) * | 2004-10-06 | 2006-10-20 | 삼성에스디아이 주식회사 | Positive type photosensitive paste composition for a PDP electrode, a PDP electrode prepared therefrom, and a PDP comprising the same |
| US20060289837A1 (en) * | 2005-06-23 | 2006-12-28 | Mcneilly Kirk | Silver salts of dicarboxcylic acids for precious metal powder and flakes |
| US20070281136A1 (en) * | 2006-05-31 | 2007-12-06 | Cabot Corporation | Ink jet printed reflective features and processes and inks for making them |
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| US20100021704A1 (en) * | 2006-09-29 | 2010-01-28 | Sung-Ho Yoon | Organic silver complex compound used in paste for conductive pattern forming |
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- 2007-01-30 KR KR1020070009177A patent/KR100709724B1/en not_active IP Right Cessation
- 2007-05-25 US US11/916,956 patent/US8088307B2/en not_active Expired - Fee Related
- 2007-05-28 CN CN2007800367362A patent/CN101523509B/en not_active Expired - Fee Related
- 2007-05-28 EP EP07746709A patent/EP2126933A4/en not_active Ceased
- 2007-05-28 WO PCT/KR2007/002561 patent/WO2008093915A1/en active Application Filing
- 2007-05-28 JP JP2009530245A patent/JP5505695B2/en not_active Expired - Fee Related
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| JPH1072673A (en) * | 1996-04-30 | 1998-03-17 | Nippon Terupen Kagaku Kk | Production of metallic paste and metallic coating |
| JP2004039379A (en) * | 2002-07-02 | 2004-02-05 | Sumitomo Electric Ind Ltd | Conductive paste, conductive membrane, and manufacturing method of conductive membrane |
| JP2003306615A (en) * | 2003-05-16 | 2003-10-31 | Asahi Glass Co Ltd | Coating solution for forming low-resistance film or low- refraction film, and method for producing the low- resistance film or low-reflection low-resistance film |
| JP2005183144A (en) * | 2003-12-18 | 2005-07-07 | Alps Electric Co Ltd | Conductive composition and manufacturing method of same |
| WO2006011180A1 (en) * | 2004-06-23 | 2006-02-02 | Harima Chemicals, Inc. | Conductive metal paste |
| JP2006049147A (en) * | 2004-08-05 | 2006-02-16 | Shoei Chem Ind Co | Conductive paste |
| JP2006183072A (en) * | 2004-12-27 | 2006-07-13 | Namics Corp | Silver particulate, method for producing the same and conductive paste containing silver particulate |
| WO2006093398A1 (en) * | 2005-03-04 | 2006-09-08 | Inktec Co., Ltd. | Conductive inks and manufacturing method thereof |
| JP2006332051A (en) * | 2005-05-23 | 2006-12-07 | Samsung Electro-Mechanics Co Ltd | Conductive ink, preparation method thereof and conductive board |
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Cited By (7)
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| JP2011243394A (en) * | 2010-05-18 | 2011-12-01 | Jsr Corp | Conductive member forming paste and forming method of conductive member |
| JP2012069273A (en) * | 2010-09-21 | 2012-04-05 | Hitachi Chem Co Ltd | Material for forming conductive film and method for forming conductive film using the same |
| JP2014189680A (en) * | 2013-03-27 | 2014-10-06 | Toppan Forms Co Ltd | Silver ink composition and conductor |
| JP2020510739A (en) * | 2017-02-08 | 2020-04-09 | ナショナル リサーチ カウンシル オブ カナダ | Printable molecular ink |
| JP7277383B2 (en) | 2017-02-08 | 2023-05-18 | ナショナル リサーチ カウンシル オブ カナダ | printable molecular ink |
| WO2020004342A1 (en) * | 2018-06-25 | 2020-01-02 | 三菱マテリアル株式会社 | Silver paste and joined body production method |
| JP2020164974A (en) * | 2018-06-25 | 2020-10-08 | 三菱マテリアル株式会社 | Silver paste and method for producing the same, and method for producing joined body |
Also Published As
| Publication number | Publication date |
|---|---|
| US20100123102A1 (en) | 2010-05-20 |
| US8088307B2 (en) | 2012-01-03 |
| CN101523509A (en) | 2009-09-02 |
| EP2126933A4 (en) | 2011-07-06 |
| WO2008093915A1 (en) | 2008-08-07 |
| CN101523509B (en) | 2012-11-28 |
| JP5505695B2 (en) | 2014-05-28 |
| EP2126933A1 (en) | 2009-12-02 |
| KR100709724B1 (en) | 2007-04-24 |
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